GREEN VORTEX-ASSISTED IONIC LIQUID-BASED DISPERSIVE LIQUID-LIQUID MICROEXTRACTION FOR ENRICHMENT AND DETERMINATION OF CADMIUM AND LEAD IN WATER, VEGETABLES AND TOBACCO SAMPLES

Author(s):  
RAGAA EL-SHEIKH ◽  
WAFAA S. HASSAN ◽  
SARA H. IBRAHIM ◽  
AMIRA M. YOUSSEF ◽  
AYMAN A. GOUDA

Objective: An eco-friendly, simple and sensitive vortex-assisted ionic liquid-based dispersive liquid-liquid microextraction method (VA-IL-DLLµE) has been proposed to enrich and determine trace levels of cadmium (Cd2+ ) and lead (Pb2+ ) ions in water, vegetables and tobacco samples, prior to its FAAS determination. Methods: The proposed method based on utilization of ionic liquid (IL) (1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate [HMIM][FAP]) as an extraction solvent for both ions after the complexation with 4,5-dihydroxy-3-phenylazo-2,7-naphthalenedisulfonic acid, disodium salt (Chromotrope 2R) at pH 6.5. The impact of different analytical parameters on microextraction efficiency was optimized. Results: In the ranges of 1.0–300 and 2.0-400 μg/ml, the calibration graphs were linear. The limits of detection were 0.3 and 0.6 μg/ml for Cd2+ and Pb2+ ions, respectively. The preconcentration factor was 100. The relative standard deviation (RSD %)<3.0%, which indicates the proposed method has high precision. Conclusion: The proposed VA-IL-DLLµE method was developed and applied for the estimation of Cd2+ and Pb2+ ion content in various water, vegetables and tobacco samples, and satisfactory results were obtained. The obtained recovery values showed good agreement with the certified values.

2014 ◽  
Vol 675-677 ◽  
pp. 181-184 ◽  
Author(s):  
Gui Qi Huang ◽  
She Ying Dong ◽  
Zhen Yang ◽  
Ting Lin Huang

An ultrasound-assisted ionic liquid based dispersive liquid-liquid microextraction (UA-IL-DLLME) was developed for the determination of four plant hormones (6-benzyladenine (6-BA), kinetin (6-KT), 2, 4-dichlorophenoxy acetic acid (2, 4-D) and uniconazole (UN)) in soil, using high performance liquid chromatography (HPLC)-diode array detection (DAD). Several important parameters including the type and volume of extraction solvent, the volume of disperser solvent, ultrasound time, pH of the solution and salt effect were studied and optimized. Under optimum conditions, the limits of detections (LODs) for the target analytes were in the range of 0.002-0.01 μg g-1. And satisfactory recoveries of the target analytes in the soil samples were 79.3-96.7 %, with relative standard deviations (RSD, n=5) that ranged from 4.3 to 6.7%.


Author(s):  
RAGAA EL SHEIKH ◽  
MOHAMMED ABDULLAH ATWA ◽  
AMIRA ATEF ABDULLAH ◽  
ANDAYMAN ABOU ELFETOUH GOUDA

Objective: Green, easy, and sensitive vortex-assisted ionic liquid-based dispersive liquid–liquid microextraction technique (VA-IL-DLLME) was developed to preconcentrate and determine trace quantities of cadmium (Cd2+) ions from real food samples, before detection by flame atomic absorption spectrometry. Methods: The proposed technique base on the utilization of IL (1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate) as an extraction solvent for Cd2+ ions after the complexation with 2-(2’-benzothiazolylazo) chromotropic acid at pH 8.0. The impact of different analytical parameters on microextraction efficiency was investigated. The validation of the proposed procedure was verified by the test of certified reference material (SRM spinach leaves 1570A) applying the standard addition method. Results: In the range of 1.0–300 μg/L, the calibration graph was linear. Limit of detection, preconcentration factor and the relative standard deviation (RSD%, 25, 150, and 250 μg/L, n=5) were 0.2 μg/L, 100, and 2.0–3.2%, respectively. Conclusion: Green, VA-IL-DLLME method was developed and applied to preconcentrate and determine of trace quantities of Cd2+ in real food samples with satisfactory results. The obtained recovery values showed good agreement with the certified values.


2019 ◽  
Vol 84 (4) ◽  
pp. 435-443 ◽  
Author(s):  
Oya Urucu ◽  
Ece Yetimoglu ◽  
Seyda Donmez ◽  
Sabahattin Deniz

An eco-friendly, simple, and sensitive solidification of floating organic drop based dispersive liquid?liquid microextraction (SFODME) procedure was introduced for the separation and preconcentration of cadmium. After 2-(5-bromo- -2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was complexed with cadmium ions in sample, the undecanol?ethanol?water ternary system was used as an organic solvent for extraction. The main factors relevant to the microextraction efficiency such as pH, concentration of 5-Br-PADAP, amount of extraction solvent were optimized. The detection limit is 0.01 ?g L-1 along with preconcentration factor 266. The recovery of the analyte was between 98 % and 103 %, with relative standard deviation below 6 %. The developed procedure was successfully tested on the analysis of water, hair dye, and food samples.


2014 ◽  
Vol 881-883 ◽  
pp. 631-634 ◽  
Author(s):  
Jian Qi Sun ◽  
Ming Tang ◽  
Jun Dai

A simple and reliable method combining dispersive liquid-liquid microextracion (DLLME) with gas chromatography (GC) using flame ionization detection (FID) was developed for the simultaneous determination of aniline (AL),o-toluidine (o-TLD),N,N-dimethylaniline (N,N-DAL),p-chloroaniline (p-CAL), andp-nitroaniline (p-NAL) in wastewater. For this purpose, dispersive liquid-liquid microextraction (DLLME) was applied as a sample preparation technique. The DLLME conditions such as the types and volume of extraction solvent, the types and volume of the disperser solvent, pH value and salt addition were studied and optimized. The method was linear in the ranges from 2.2×10-3to 100.0 μg·mL-1for aforementioned aromatic amines withR2≥ 0.9968. The DLLME procedure allowed efficient recovery of the investigated aromatic amines ranging between 82 % and 92 % with a relative standard deviation (RSD) ≤ 3.4 for actual wastewater samples spiked with 5, 10 and 20 μg·mL-1of aromatic amines, respectively. These results showed the potential of this technique for aromatic amines monitoring in wastewater samples. Furthermore, the investigated methods are simple, reproducible, and inexpensive.


2012 ◽  
Vol 518-523 ◽  
pp. 1379-1382
Author(s):  
Ying Chun Yang ◽  
Qian Sun ◽  
Chong Shu Yi ◽  
Zhi Xiang Ye ◽  
Li Mo

A rapid and effective method, the dispersive liquid-liquid microextraction(DLLME) with gas chromatography, has been developed for the extraction and determination of OCP in environmental water samples. The factors relevant to the efficiency of DLLME were investigated and optimized. Under the optimum conditions, such as 150μL of dichloromethane as extraction solvent, 1.2 mL acetone as dispersive agent, 8 minutes extraction time, and without salt addition, the linear response of this method was in the range of 0.5~5000μg L−1 (r = 0.9981), the relative standard deviation (RSD) for 500μg L−1 and 1000μg L−1 of OCP was 5.2% and 12.6% (n = 6), respectively. The detection limit (3σ) was 0.08 μg L−1. The developed method was successfully applied to the determination of trace amount of OCP in three kinds of real environmental water samples, the spiked recoveries were in the range of 87.4%~108.0%.


2014 ◽  
Vol 1030-1032 ◽  
pp. 357-360 ◽  
Author(s):  
Jian Qi Sun

This study describes an analytical method employing capillary gas chromatography (GC) using flame ionization detection (FID) that has been developed for the simultaneous determination of food preservatives in drinks, including sorbic acid (SA), benzonic acid (BA) and methyl paraben (MP). For this purpose, dispersive liquid-liquid microextraction (DLLME) was applied as a sample preparation technique. The DLLME conditions such as the types and volume of extraction solvent, the types and volume of the disperser solvent, pH value and salt addition were investigated and optimized. The method was linear in the ranges from 0.5 to 100.0 μg·mL-1for abovementioned preservatives withR2≥ 0.9991. The DLLME procedure allowed efficient recovery of the analyted preservatives ranging between 91 % and 108 % with a relative standard deviation (RSD) ≤ 6.1 for the blank samples spiked with 20, 40 and 80 μg·mL-1of preservatives, respectively. The developed procedure was demonstrated to be a effective method for the analysis of preservatives in drinks. Furthermore, the method is simple, reproducible, envioronmentally friendly and inexpensive.


2013 ◽  
Vol 67 (2) ◽  
pp. 247-253 ◽  
Author(s):  
Zonghao Li ◽  
Gong Yu ◽  
Jun Song ◽  
Qi Wang ◽  
Mousheng Liu ◽  
...  

A new, simple and rapid method based on dispersive liquid–liquid microextraction (DLLME) was developed for extracting and preconcentrating copper (Cu), nickel (Ni), lead (Pb) and cadmium (Cd) in water samples prior to flame atomic absorption spectrometry (FAAS) analysis. 1-(2-thiazolylazo)-naphthol (TAN) was used as chelating reagents, and non-ionic surfactant Triton X-114 and CCl4 as disperser solvent and extraction solvent, respectively. Some influential factors relevant to DLLME, such as the concentration of TAN, type and volume of disperser and extraction solvent, pH and ultrasound time, were optimized. Under the optimal conditions, the calibration curve was linear in the range of 10–800 μg L−1 for Cu and Ni, 10–500 μg L−1 for Pb, and 10–1,000 μg L−1 for Cd, respectively. The limits of detection for the four metal ions were below 0.5 μg L−1, with the enhancement factors of 105, 66, 28 and 106 for Cu, Ni, Pb and Cd, respectively. The relative standard deviations (RSD, n = 6) were 2.6–4.1%. The proposed method was applied to determination of Cu, Ni, Pb and Cd in water samples and satisfactory relative recoveries (93.0–101.2%) were achieved.


2014 ◽  
Vol 881-883 ◽  
pp. 627-630 ◽  
Author(s):  
Jian Qi Sun ◽  
Fang Zeng ◽  
Xiao Feng Liu

This study describes an analytical method employing capillary gas chromatography (GC) using flame ionization detection (FID) that has been developed for the simultaneous determination of acrylates (methyl acrylate (MA), methyl methacrylate (MMA), butyl acrylate (BA)) in wastewater. For this purpose, dispersive liquid-liquid microextraction (DLLME) was applied as a sample preparation technique. The DLLME conditions such as the types and volume of extraction solvent, the types and volume of the disperser solvent, pH value and salt addition were studied and optimized. The method was linear in the ranges from 4.3×10-4 to 200.0 μg·mL-1 for abovementioned acrylates with R2≥ 0.9992. The DLLME procedure allowed efficient recovery of the investigated acrylates ranging between 81 % and 109 % with a relative standard deviation (RSD) ≤ 9.1 for the blank samples spiked with 10, 50 and 100 μg·mL-1 of acrylates, respectively. These results showed the potential of this technique for acrylates monitoring in wastewater samples. Furthermore, the investigated methods are simple, reproducible, and inexpensive.


2020 ◽  
Vol 3 (03) ◽  
pp. 18-24
Author(s):  
Ehsan Zolfonoun

Dispersive liquid–liquid microextraction coupled with UV–Vis spectrophotometry was applied for the determination of zirconium in aqueous samples. In this method a small amount of chloroform as the extraction solvent was dissolved in pure ethanol as the disperser solvent, then the binary solution was rapidly injected by a syringe into the water sample solution containing Zr(IV), xylenol orange and cetyltrimethylammonium bromide. The formed ion-associate was extracted into the fine chloroform droplets. The detection limit for Zr(IV) was 0.010 µg mL−1. The precision of the method, evaluated as the relative standard deviation obtained by analyzing of 10 replicates, was 2.7 %. The practical applicability of the developed method was examined using natural waters and ceramic samples.


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